LC-UV和LC-MS在山楂叶多元酚类成分分析中的应用比较  

The Comparison between LC-UV and LC-MS in Analysis of Polyphenolic Components from Leaves of Crataegus L.

作　　者：刘荣华[1] 江爱龙 弁玲丽[3] 邵峰[1] 马志林[1] 余伯阳[3] 

机构地区：[1]江西中医学院现代中药制剂教育部重点实验室,江西南昌330004 [2]武警江西省总队医院,江西南昌330030 [3]中国药科大学中药复方研究室,江苏南京210038

出　　处：《中药材》2007年第3期285-289,共5页Journal of Chinese Medicinal Materials

基　　金：国家自然科学基金资助项目(No.30472161);江西省自然科学基金资助项目(No.0640163)

摘　　要：目的:对LC-UV和LC-MS在山楂叶多元酚类成分分析中的应用进行方法学比较。方法:采用高效液相色谱并联双检测器(VWD和MSD)法。色谱柱为Lichrospher C18(250×4.6 mm I.D.,5μm);流动相A为乙腈,B为0.5%甲酸溶液,梯度洗脱,0-12 min A由11%-17%,12-30 min A由17%-18%,30-45 min A由18%-40%,45-60 minA由40%-100%;流速为1ml/min,三向分流阀分流进入MSD和VWD进行检测;柱温30℃;进样量10μl。结果:LC-MS灵敏度比HPLC法高10倍以上,在检测样品中微量成分时具有很大的优势;另外,LC-MS是根据tR和m/z两项指标来确定成分的类型,对于某些用LC-UV方法不能得到良好分离的组分或在LC-UV图谱上保留时间与对照品相近的其它成分,可以选用选择性离子检测(SIM)进行分析,能避免这些成分的干扰,因而具有高度的选择性和专属性。而LC-UV法操作简便,成本低,流动相选择面较广,因而分离度往往比LC-MS高,在检测样品中具有较好的紫外吸收、较好的分离度以及含量较高的成分时,LC-UV法以其高精密度和高稳定性完全可以达到LC-MS同样的检测结果。结论:LC-MS和LC-UV在山楂叶多元酚类成分的定量分析方面各有特色,可根据不同的检测指标选用不同的检测器。Objective ： To compare the analytical method of LC-UV and LC-MS determination of major polyphenolic components in leaves of Crataegus L. Methods： By high-performance liquid chromatography method with VWD and MSD, Liehropsher C18 column （ 250 × 4. 6 mm I. D. , 5 μm） ; mobile phase consisted of solvent A （acetonitrile） and solvent B （0. 5 % formic acid） ; elution profile was： 0-12 min 11% to 17% A in B（linear gradient）, 12-30 min 17% to 18% A in B（linear gradient）, 30-45 min 18% to40% A in B（linear gradient）, 45-60 min 40% to 100% A in B（linear gradient） ; flow rate was 1.00 ml/min, flow into MSD and VWD by diffluence, column temperature 30℃ and the injection volume 10 μl. Result： The sensitivity of LC-MS was 10 times more than that of LC-UV, so it is preponderance for mieroanalysis. Additionally, because LC-MS can identify the component by retention time（tR ） and m/z, it has high selectivity and exclusion for the determined component. However, the method of LC-UV is simple; the cost is lower; the separate effect is better. So it is preponderance to determine the higher content component, which has better separate effect. Conclusion： LC-UV and LC-MS exhibited their own predominance for determination of major polyphenolie components in leaves of Crataegus L. So the detector should be selected according to the determined targets.

关 键 词：LC—MS LC—UV HPLC 山楂叶 多元酚 

分 类 号：R284.1[医药卫生—中药学]